Refinement of vitamin-containing unsaponifiable matter of oils



Patented Dec. 11,1934

PATENT OFFICE BEFINEMENT F UNSAPONIFIABLE Archie Black, New Brunswick, N. 1.,

E. R. Squibb a Sons, New York, N.

poration oi New York vrrsmN-oon'rammo mm or one anignor to 1., a cor- No Drawing. Application April 2:, 1932.

Serial No. 600.904

comm. (0!. 167-81) This invention relates to the refinement oi the vitamin-containing unsaponiflable matter of oils.

In the processes commonly employed, the vitamin-containing unsaponiflable 'matter of oils is 5 isolated by the successive steps of saponiiying the oil, extracting the soap with a solvent in which the unsaponifiable matter dissolves but the soap does not, removing the solvent from the extract by evaporation, and removing most of the cholesterol from the extract by crystallization from a solvent. There remains a semi-solid brown mass, the crude unsaponifiable matter.

It is theobject of this invention to provide a simple and eflicient method of refining such unsaponiflable matter so as to obtain a product characterized by higher concentration of vitamins and by increased palatability in virtue of superior flavor, odor, and color.

Essentially the method of the invention comprises dissolving the unsaponiflable matter in a solvent not procured from petroleum, preferably a solvent selected from the group consisting of ether, benzol, chloroform, and alcohol; and treating the solution anaerically with an adsorbent, preferably an adsorbent selected from the group consisting of carbons of vegetable and animal origin and earths. Such treatment may be variously effected, as by agitating the solution with, or percolating it through a bed of, the adsorbent. Preferably a small amount of an antioxidant, say hydroquinone or pyrogallol, is added to the solution, and the adsorbent is freed of oxygen, before the treatment. Such treatment, which entails the loss of only a negligible quantity of vitamins, not only eliminates from the unsaponiflable matter a large proportion of the inert substances, but also makes it far more acceptable for human consumption.

As an eiilnpla 60 g. of carbon is placed in a percolator d covered with ether, the system is flooded wi carbon dioxide, and the carbon is washed with ether containing a small amount of hydroquinone. To a 300 cc. ether solution of the unsaponifiable matter of 4000 g. of cod-liver oil, 5 g. of hydroquinone is added; and the solution is then drawn, by means or a low vacuum, through the bed or carbon. The carbon is washed with tour 100 cc. portions of ether, and the washings are added to the main solution of the unsaponiflable matter; and the solution is washed with dilute aqueous sodium hydroxide solution to remove the hydroquinone, and is concentrated in vacuo. The residue weighs only percent as much as the crude unsaponifiable mat-, 5 ter, is much lighter in color and has a markedly better flavor and odor, and is found by biological and color tests to contain substantially all the original vitamins A and D.

It is to be understood that the foregoing embodiment is merely illustrative and by no means limitative of the invention, which may assume various other forms-as to particular substances, proportions, and procedureswithin the scope of the appended claims.

I claim:

1. The method of refining the vitamin-containing unsaponiflable matter of oils so as torecover and protect substantially the entire vitamins A and D content thereof that comprises dissolving such unsaponiflable matter in a solvent not procured from petroleum, treating the solution anaerically with an adsorbent, in the presence of an antioxidant, and discarding the adsorbent together with the impurities carried thereby.

2. The method of refining the vitamin-containing unsaponiflable matter of oils so as to recover ahd protect substantially the entire vitamin A- and D content thereof that comprises dissolving such unsaponiflable matter in a solvent selected from the group consisting of ether, benzol, chloroform, and alcohol; treating the solution anaerically with an adsorbent selected from the group consisting of carbons of vegetable and ani- 35 mal origin and earths, in the presence of an antioxidant selected from the group consisting of hydroquinone and pyrogallol, and discarding the adsorbent together with the impurities carried thereby.

3. The method uns'aponiflable matter 40 of refining vitamin-containing oi oils so as to recover and protect substantially the entire vitamin A and D content thereof that comprises dissolving such unsaponiflable matter in ether, treating the solu- 45 tion anaerically with carbon, in the presence of hydroquinone, and discarding the carbon together with the impurities carried thereby,

. ARCHIE BLACK. 9 

